Living with breakthrough: Two-dimensional liquid-chromatography separations of a water-soluble synthetically grafted bio-polymer

H. C. van de Ven*, J. Purmova, G. Groeneveld, Tijmen S. Bos, A. F.G. Gargano, Sj van der Wal, Y. Mengerink, Peter J. Schoenmakers

*Corresponding author for this work

Research output: Contribution to JournalArticleAcademicpeer-review

Abstract

In this study, we evaluate the use of various two-dimensional liquid chromatographic methods to characterize water-soluble, synthetically grafted bio-polymers, consisting of long poly(acrylic acid) chains and short maltodextrin grafts. The confirmation of the presence of grafting and the estimation of its extent is challenging. It is complicated by the limited solubility of polymers, their structural dispersity and chemical heterogeneity. Moreover, the starting materials (and other reagents, reaction products and additives) may be present in the product. Reversed-phase liquid chromatography (RPLC), hydrophilic-interaction liquid chromatography (HILIC) and size-exclusion chromatography (SEC) were used to characterize the product, as well as the starting materials. Additionally, fractions were collected for off-line characterization by infrared spectroscopy and mass spectrometry. The one-dimensional separation methods were found to be inconclusive regarding the grafting question. Breakthrough (the early elution of polymer fractions due to strong injection solvents) is shown to be a perpetual problem. This issue is not solved by comprehensive two-dimensional liquid chromatography (LC × LC), but information demonstrating the success of the grafting reaction could be obtained. SEC × RPLC and HILIC × RPLC separations are presented and discussed.

Original languageEnglish
Article number41
Pages (from-to)1-16
Number of pages16
JournalSeparations
Volume7
Issue number3
Early online date15 Jul 2020
DOIs
Publication statusPublished - Sep 2020

Keywords

  • Breakthrough
  • Grafted bio-polymer
  • HILIC × RPLC
  • LC × LC
  • Polyacrylic acid–maltodextrin hybrid
  • SEC × RPLC

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